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By Richard O. Carlson

Ions of p31 and B 11 were implanted in natural insulating diamond macles. The thin (-0.4µ) layers showed sheet resistances of 107 to 1011 ohm per sq and activation energies of 0.17 to 0.34 ev above room temperature. However, no Hall effect could be measured, indicating that mobilities were less than I to 10 sq cm per (v-sec). Such low mobilities may be due to excessive scattering due to radiation damage in the bombarded layer or to very high concentrations of active compensating impurities. Annealing did not materially change the room -temperature properties, but the temperature was limited to -800°C by surface graphitization, the latter process probably being accelerated by lattice damage in our diamonds arising from the ion bombardment. A weak n-type thermoelectric power was detected after p31 irradiation, but it cannot be presumed that we have made the phosphorus ions active as donors in diamond. The natural diamonds have a high and uncontrolled concentration of impurities and, when coupled with the radiation damage and graphitization problems, would appear to seriously limit the quality of semiconductor that we can presently achieve by ion implantation in diamond. ALTHOUGH diamonds are usually thought of as insulating in terms of their electrical conductivity, it was found about 15 years ago that natural semiconducting diamonds do occur rarely, and these were designated as type IIb diamonds. These p-type semiconducting diamonds were found to be dominated by an impurity level 0.37 ev from the valence band. Evidence today based on correlation of the concentration of acceptor states from Hall effect measurements with the impurity concentrations determined by neutron activation analysis point to aluminum as the dominant acceptor impurity.' The compensating donor is believed to be nitrogen, which has a donor level 1.6 ev above the valence band.' However, only a small fraction of the total nitrogen content in the diamond is electrically active. An infrared absorption band at 7.8 p and ultraviolet absorption near 4 ev have been associated with nitrogen, the former providing a quantitative measure of nitrogen content.3 The nitrogen content is -l020 cm-3 in insulating or type I diamonds, but is less than 10'' in natural semiconducting diamonds. Much of this nitrogen is distributed in platelets oriented in (100) planes and not atomically dispersed in the diamond lattice.4 Semiconducting diamonds have been deliberately formed by incorporating impurities into the graphite charge in the high-pressure apparatus used to form diamonds.5 These manufactured semiconducting diamonds are always p-type, and while some show the 0.37 ev level due to aluminum, most such samples have been ascribed to impurity banding effects.6 The best natural or manufactured semiconducting diamonds have hole mobilities near 1500 sq cm per (v-sec) at room temperature, and those with the 0.37-ev level can be analyzed to reveal an acceptor concentration of 3 to 8 X 1016 cm-3 and a donor concentration 3 to 10 times lower.' NO bulk n-type diamonds have ever been reported, but the electron mobility has been measured as 1900 sq cm per (v-sec) by irradiating a diamond with ultraviolet to excite electrons out of the deep nitrogen donor level or other levels.7 New hope for the formation of n-type diamond has emerged from the ion-implantation method whereby desired impurities are introduced into a crystal lattice by bombardment with a high-energy beam of the impurity ion. It was found in the case of silicon that the usual donors such as phosphorus and arsenic and acceptors such as boron and gallium could be implanted into silicon. Wentorf and arrow' produced semiconducting layers on diamonds by an ionic bombardment in a glow discharge at potentials of about 2 kv. The observed typeness from thermoelectric probing seemed to depend on the atmosphere gas (nitrogen, argon, or hydrogen) rather than on the electrode material, but the nature of the conduction process in the thin damaged surface layer is completely unknown. A Russian group under Vavilov has attempted high-energy ion implantation in natural diamonds using boron and lithium ions9 and later also phosphorus, aluminum, and carbon ions.10 Their papers claim n-type layers from lithium, phosphorus, and carbon implant and a p-type layer from boron and aluminum implant, though the methods of type determination are not described in detail. Under government contract support, the Ion Physics Corp. has studied ion implantation in several semiconductors. While the bulk of their study1' was devoted to the irradiation of silicon, they did carry out a short study on boron and phosphorus implantation into natural diamonds. They did observe surface conducting layers but did not determine the typeness of the layers. For our experiments, phosphorus and boron were chosen as the dopant ions because of their respective donor and acceptor behavior in germanium and silicon. Moreover, they are the lightest mass dopants of the shallow level donors and acceptors from columns 111 and V of the Periodic Table (excluding nitrogen which is already present in diamond), and will have the largest depth penetration into the diamond lattice. EXPERIMENTAL Diamonds. As the target diamonds for our ion implantation study, we chose commercially available macles, which are flat, twinned diamond crystals. By scanning through the stock of a wholesale distributor

Jan 1, 1970

By Paul A. Beck

THE occurrence of the (100) [lOO] or "cube" texture upon annealing of cold-rolled copper has been much investigated.' The conditions favorable for its formation were found to be a high final annealing temperaturez or long annealing time," a high reduction of area in cold rolling prior to the final anneal,' and a small penultimate grain size." The effects of penultimate grain size and of rolling reduction were found by Cook and Richards4 to be interrelated in such a way that any combination of them giving lower than a certain value of the final average thickness of the grains in the rolled material leads to a fairly complete cube texture with a given final annealing time and temperature. Also, according to the same authors, at a higher final annealing temperature a larger average rolled grain thickness, i.e., a lower final rolling reduction, is sufficient than at a lower temperature. These somewhat involved conditions can be understood readily on the basis of recent results obtained at this laboratory. Hsun Hu was able to show recently by means of quantitative pole figure determinations that the rolling texture of tough pitch copper, which is almost identical with that of 2s aluminum: may be described roughly as a scatter around four symmetrical "ideal" orientations not very far from (123) [112]. In the case of aluminum, annealing leads to retain-ment of the rolling texture with some decrease of the scatter around the four "ideal" orientations, and to the appearance of a new texture component, namely the cube texture." A microscopic technique, revealing grain orientations by means of oxide film and polarized light, showed that the retainment of the rolling texture is achieved through two different mechanisms operating simultaneously, namely "re-crystallization in situ," and the formation of strain-free grains in orientations different from their local surroundings, but identical with that of another component of the rolling texture. Thus, a local area in the rolled material, having approximately the orientation of one of the four "ideal" components of the texture, partly retains its orientation during annealing, while recovering from its cold-worked condition, and it is partially absorbed at the same time by invading strain-free grains of an orientation approximately corresponding to that of another "ideal" texture component. The reorientation here, as well as in the formation of the strain-free grains of "cube" orientation, may be described as a [Ill] rotation of about 40°, see Fig. 1 of ref. 6. The preferential growth of grains in such orientations is a result of the high mobility of grain boundaries corresponding to this relative orientation.' " It appears very likely that in copper the mechanism of the structural changes during annealing is similar to that observed in aluminum (except for the much greater frequency of formation of annealing twins in copper). In both metals the new grains of cube orientation have a great advantage over the new grains with orientations close to one of the four components of the rolling texture. This advantage stems from their symmetrical orientation with respect to all four retained rolling texture components of the matrix; they are oriented favorably for growth at the expense of all of these four orientations. As a result, the growth of the "cube grains" is favored over the growth of the others, as soon as the new grains have grown large enough to be in contact with portions of the matrix containing elements of more than one, and preferably of all four component textures. It is clear that this critical size is smaller and, therefore, attained earlier in the annealing process if the structural units, such as grains and kink bands, representing the four matrix orientations are smaller, i. e., if the average thickness of the rolled grains is smaller. Hence, for a given annealing time and temperature, a smaller penultimate grain size and a higher rolling reduction both tend to increase that fraction of the annealing period during which the above condition is satisfied. Consequently, the percentage volume of material assuming the cube orientation increases. The same is true also for increasing time and temperature of annealing when the penultimate grain size and the final rolling reduction are constant, since the average size attained by the new grains during annealing increases with the annealing time and temperature. For the same reason, at higher annealing temperatures a given volume percentage of cube texture can be obtained with larger rolled grain thickness (larger penultimate grain size, or smaller rolling reduction) than at lower annealing temperatures. The well-known conspicuous sharpness of the cube texture may be interpreted as a result of the fact that selective growth of only those grains is favored that have an orientation closely symmetrical with respect to all four components of the deformation texture and exhibit, therefore, a high boundary mobility in contact with each. The effect of alloying elements in suppressing the cube texture, as described by Dahl and Pawlek,' appears to be associated with a change in the rolling texture. For face-centered cubic metals, such as copper, which do exhibit the cube texture upon annealing, the rolling texture is always of the type described above, i. e., scattered around four "ideal orientations" of approximately (123) [112]. The addition of certain alloying elements, such as about 5 pct Zn or 0.05 pct P in copper, has the as yet unexplained effect of changing the rolling texture into the (110) 11121 type. This texture consists of two fairly sharply developed, twin related components. In such cases, as in 70-30 brass and in silver, the annealing texture again is related to the rolling texture by a [lll] rotation of about 30°, however, because of the different rolling texture to start from, it has no cube texture component. At higher temperatures, both in brassm and in silver," grain growth leads to a further change in texture: A [lll] rotation of the same amount, but in reversed direction, back to the original rolling texture.

Jan 1, 1952

By Notman, Arthur

THIS is a day of surpluses, some good and some not so good. One can hardly pick up a newspaper, magazine, review or economic treatise without confronting the fact that we have or are threatened with more .of certain goods than we have use for, whether it be corn, wheat, cotton, coal or oil, -lumber, 'leather, newsprint, automobiles, zinc, lead, copper or what not. How did this unprecedented state of affairs arise? Who is to blame? How shall we avoid smothering ourselves in our own production? The voice of the farmer is raised in appeal to the Government to relieve him from the dilemma of his own fertility. In answer the Government employs thousands of experts and spends millions of dollars to aid the farmer. But to what end? To make him still more efficient so that he may produce even greater surpluses? Not satisfied with the result, it spends other millions to prepare vast areas of the arid land of the West for more farmers to cultivate and insure yet larger surpluses. Then what? Naturally another appeal to the Government to fix prices by financing the

Jan 1, 1928

By Northcutt Ely

This chapter deals with the systems of laws by which governments regulate the exploration for and production of the minerals within their jurisdictions. It is a summary, restricted by necessary space limitations, of material assembled by the author for a publication of the United States Bureau of Mines, "Summary of Mining and Petroleum Laws of the World," (Information Circular 80 1 7, 196 1. ) The present study is organized in three parts, dealing with (1) the historical background of these legal systems, (2) laws of the United States, and (3) laws of other countries of the world. The reader's attention is invited to the acknowledgments at the end of the chapter, which inadequately express the appreciation due those who have assisted in the collection of this material. Part I. Historical Development of Major Western Systems of Land Tenancy with Respect to the Ownership and Control of Minerals The use of metals in primitive societies was largely confined to the manufacture of weapons for self-preservation. The ruler's control over copper, then bronze, then iron, was essential to maintenance of his own ascendancy at home and his group's position against neighbors who had access to similar metals. Ancient societies were thus characterized by the ruling group's ownership of minerals and metals. The Egyptian civilization, which emerged in the fourth millenium B.C. upon the agricultural subjugation of the lower valley of the Nile, was responsible for extensive development of the upper valley as a source of mineral wealth. The production of gold during the height of that civilization has been estimated at $30,000,000 per year, thus equaling the early placers of California and Australia. The mines of Egypt were the property of the Pharaohs and were controlled at their direction. Greek mining developed a different scheme of land tenancy which more closely resembled modem concepts. Development of mineral resources was

Jan 1, 1964

By Earnshaw Cook, H. S. Avery, J. A. Fellows

TEe increased use of heat-resistant alloys (26 per cent Cr, 12 per cent Ni; 16 per cent Cr, 35 per cent Ni; 12 per cent Cr, 60 per cent Ni; etc.) in recent years has been accompanied by continued demands by the consumer for improvement in properties. The manufacturers of these materials, of necessity, have resorted to more critical studies of the basic causes of variations in fundamental properties. To keep pace with the need for augmented information, previous techniques of investigation have been refined and new test methods and instruments created. It is the purpose of this paper to describe the apparatus, experimental technique and precision of measurement that were employed in the exploration of properties of heat-resistant alloys presented in a companion paper. The detailed precautions in experimental procedure essential for attainment of accurate and comparable data at elevated temperatures cannot be too highly emphasized. The Creep Test Since the fundamental concepts of creep testing have been recognized for the past 20 years, present interest is restricted to refinements in equipment and experimental procedure. The creep-test iaboratory constructed for the American Brake Shoe and Foundry Co. is designed to permit I000-hr. tests in the temperature range of I200° to 2 200°F. with a choice of applied stress extending from jo to 50,000 lb. per sq. in. in increments of 50 lb. per sq. in. To simplify the calculation of weight combinations, the loading beams (Fig. I) are provided with counterweights to eliminate the tare. The precision of the knife-edges (10:I ratio) is such that a 10-gram weight placed on the upper specimen grip will be exactly balanced by a I-gram weight attached to the loading shackle. Check of the loading weights proved the maximum error to be 0.06 per cent. Axial alignment is provided by crossed knife-edges in the grip seats. The furnaces are similar in design to those of Crane and Company, Battelle Memorial Institute, and the U.S. Steel Corporation. An 80 per cent Pt, zo per cent Rh No. 19 B. and S. gauge wire is used as the heating element. The details of -construction are shown in the radiograph reproduced in Fig. 2. The windings are held in place on an alundum tube with aludum cement; the distribution of turns is adjusted to give a maximum temperature gradient of , I°F. over a 4-in. gauge length (Fig. 3). To avoid sharp temperature differentials at the ends of the test section, the length of the furnace is four times the gauge length. Sixteen-inch coupons are used „ to reduce the temperature of the threaded joints and thus to facilitate removal from the grips. Thermal losses are minimized by refractory insulators cut to shape and surrounded by diatomaceous ear,th. The taps

Jan 1, 1942

By J. A. Fellows, Earnshaw Cook, H. S. Avery

TEe increased use of heat-resistant alloys (26 per cent Cr, 12 per cent Ni; 16 per cent Cr, 35 per cent Ni; 12 per cent Cr, 60 per cent Ni; etc.) in recent years has been accompanied by continued demands by the consumer for improvement in properties. The manufacturers of these materials, of necessity, have resorted to more critical studies of the basic causes of variations in fundamental properties. To keep pace with the need for augmented information, previous techniques of investigation have been refined and new test methods and instruments created. It is the purpose of this paper to describe the apparatus, experimental technique and precision of measurement that were employed in the exploration of properties of heat-resistant alloys presented in a companion paper. The detailed precautions in experimental procedure essential for attainment of accurate and comparable data at elevated temperatures cannot be too highly emphasized. The Creep Test Since the fundamental concepts of creep testing have been recognized for the past 20 years, present interest is restricted to refinements in equipment and experimental procedure. The creep-test iaboratory constructed for the American Brake Shoe and Foundry Co. is designed to permit I000-hr. tests in the temperature range of I200° to 2 200°F. with a choice of applied stress extending from jo to 50,000 lb. per sq. in. in increments of 50 lb. per sq. in. To simplify the calculation of weight combinations, the loading beams (Fig. I) are provided with counterweights to eliminate the tare. The precision of the knife-edges (10:I ratio) is such that a 10-gram weight placed on the upper specimen grip will be exactly balanced by a I-gram weight attached to the loading shackle. Check of the loading weights proved the maximum error to be 0.06 per cent. Axial alignment is provided by crossed knife-edges in the grip seats. The furnaces are similar in design to those of Crane and Company, Battelle Memorial Institute, and the U.S. Steel Corporation. An 80 per cent Pt, zo per cent Rh No. 19 B. and S. gauge wire is used as the heating element. The details of -construction are shown in the radiograph reproduced in Fig. 2. The windings are held in place on an alundum tube with aludum cement; the distribution of turns is adjusted to give a maximum temperature gradient of , I°F. over a 4-in. gauge length (Fig. 3). To avoid sharp temperature differentials at the ends of the test section, the length of the furnace is four times the gauge length. Sixteen-inch coupons are used „ to reduce the temperature of the threaded joints and thus to facilitate removal from the grips. Thermal losses are minimized by refractory insulators cut to shape and surrounded by diatomaceous ear,th. The taps

Jan 1, 1942

By J. A. Fellows, Earnshaw Cook, H. S. Avery

THE increased use of heat-resistant alloys (26 per cent Cr, 12 per cent Ni; 16 per cent Cr, 35 per cent Ni; 12 per cent Cr, 60 per cent Ni; etc.) in recent years has been accompanied by continued demands by the consumer for improvement in properties. The manufacturers of these materials, of necessity, have resorted to more critical studies of the basic causes of variations in fundamental properties. To keep pace with the need for augmented information, previous techniques of investigation have been refined and new test methods and instruments created. It is the purpose of this paper to describe the apparatus, experimental technique and precision of measurement that were employed in the exploration of properties of heat-resistant alloy presented in a companion paper.? The detailed precautions in experimental procedure essential for attainment of accurate and comparable data at elevated temperatures cannot be too highly emphasized. THE CREEP TEST Since the fundamental concepts of creep testing have been recognized for the past 20 years, present interest is restricted to refinements in equipment and experimental procedure. The creep-test laboratory constructed for the American Brake Shoe and Foundry Co. is designed to permit 1000-hr. tests in the temperature range of 1200° to 2200°F. with a choice of applied stress extending from 50 to 50,000 lb. per sq. in. in increments of 50 lb. per sq. in. To simplify the calculation of weight combinations, the loading beams (Fig. I) are provided with counterweights to eliminate the tare. The precision of the knife-edges (10.1 ratio) is such that a 10-gram weight placed on the upper specimen grip will be exactly balanced by a 1-gram weight attached to the loading shackle. Check of the loading weights proved the maximum error to be 0.06 per cent. Axial alignment is provided by crossed knife-edges in the grip seats. The furnaces are similar in design to those of Crane and Company, Battelle Memorial Institute, and the U.S. Steel Corporation. An 80 per cent Pt, 20 per cent Rh No. 19 B. and S. gauge wire is used as the heating element. The details of construction are shown in the radiograph reproduced in Fig. 2. The windings are held in place on an alundum tube with alundum cement; the distribution of turns is adjusted to give a maximum temperature gradient of ± 1°F. over a 4-in. gauge length (Fig. 3). To avoid sharp temperature differentials at the ends of the test section, the length of the furnace is four times the gauge length. Sixteen-inch coupons are used to reduce the temperature of the threaded

Jan 1, 1942

By D. B. RUSHNORE, K. A. Pauly

Bulletin. No. 41, May, 1910. ABBREVIATIONS. Al. Ind., Alliance Industrielle. am. Elec'n.. . American. Electrician. Bull. As. Ing. El Bulletin de la Association des Ingenieurs Elec- triciens Sortis de l'Institut Electrotecnique Montefiore, Liege. Bull. Soc. bilge d' Elec Bulletin de la Société belge d'Electriciens. Col. Guard . Colliery Guardian. D. R. P Deutsches Reich Patent. Dilly. Poly Dingler's Polytechniches Journal. E. & DI. Jour Engineering and Mining Journal. E. T. Zeit Electrotechnische Zeitschrift. Eclair. Elec. L'Eclairage Electrique. 1;1. Anzeig Elektrotechnischer Anzeiger

Sep 1, 1910

By AIME AIME

ARRANGEMENTS for the Annual Meeting of the Institute were well advanced at the end of December as the following program will show. Heretofore this has been printed separately, but its inclusion in the Annual Review issue of MINING AND METALLURGY will, it is hoped, make it more easily available for reference until the final program is issued, which will be distributed at the meeting. Added details will appear in the February issue. Last year's meeting drew a record crowd of over 2300 which should be exceeded this year. Early reservations at the headquarters hotel, the Waldorf-Astoria, or any other convenient hotel are desirable, as are prompt reservations for the Annual Dinner. No one need worry about too much speechmaking this year, for the honors will be awarded and accepted in a few words instead of a few paragraphs, in seconds rather than minutes.

Jan 1, 1939

By W. D. Forgeng, B. F. Decker

IT has been known for almost a century' that silicon and nitrogen combine when heated to a high temperature. Three nitrides have been reported, SiN, Si3N,, and Si,N, containing 33.3, 40.0 and 42.9 pct nitrogen by weight, respectively. The existence of SisN, is well established but that of Si,N, and SiN is doubtful. The first systematic study of the reaction between silicon and nitrogen was made in 1910 by Weiss and Engelhart" who determined the rate at which silicon absorbed nitrogen at temperatures from 1250°C to

Jan 1, 1959

Jan 1, 1962

By Nathan C. Rockwood

WHILE mining engineers have been searching in far corners of the country and of the world for hidden wealth there has grown up around us in nearly every city great wealth-producing mines calling for the investment of hundreds of millions of dollars and yielding products now sold for over half a billion dollars yearly-largely unknown and almost wholly neglected by mining engineers. But this neglect is explainable and excusable. They are industries of very recent origin-practically the growth of the last 25 years. They are in a very large measure the result of tremendous developments in engineering construction and the rapidly expanding use of portland cement concrete for structures of every description. Concrete as a material of construction is going through an evolution very much as did cast iron and other metals used in engineering; and this phase of the industry should appeal to the imagination of metallurgical engineers. At first iron was iron-a material of uncertain properties, owing both to small differences in chemical composition and in methods of manufacture. By successive steps iron was studied and knowledge of its properties developed-the striking effects of very small percentages of other minerals and of various heat-treatments.

Jan 1, 1924

By Leo Ranney

ANY years ago a prospector came to a Nevada town and built himself a shack. Day after day he searched the hills for gold -but he found none. He closed his shack and hurried north, where a strike had been made. Next he tried to trap the flour gold that floats down the Snake River. He panned the black sands along the Oregon coast. He ranged over the mountains and up the gulches of far-off Alaska. At last, broken in health, six years ago he came back to his old home in Nevada. There his shack still stood-nobody wanted it. One day he started a garden in the rocky soil that he owned. His spade turned up a chunk of quartz, and in that quartz were stringers of gold. He had found a rich gold vein, running right under his own house. You gas producers who have hurried to Oklahoma, Louisiana, East Texas, South Texas, West Texas, even to California to drill wildcat holes a mile or two miles deep-why not, like the old gold prospector, have a look in your own back yard? Some of your coal seams contain 20,000,000 cu. ft. of natural gas per acre.

Jan 1, 1943

By A. CHESTER BEATTY

MAGNESIUM oxide is by far the most refractory of the common oxides, since it has a melting point of 5072 deg. F. as compared with 3110 deg. F., the melting point of silica (crystobalite) ; 3722 deg. F., the melting point of alumina (corundum) ; and 4127 deg. F., the melting point of chromite (Cr2O33FeO). Its large-scale use in the lining of metallurgical furnaces dates back to the latter part of the nineteenth century, when extensive deposits of magnesium carbonate were discovered in southern Austria in the province of Styria. Before the development of Austrian magnesite, calcined dolomite, a mixture of lime and magnesia, was used in basic steel-making furnaces. The lime in the dolomite was quite objectionable, since it slaked on exposure to the atmosphere, and dolomite therefore could not be made' .into permanent furnace bottoms or into brick. The Austrian magnesite, with its very low lime content, was free from these objections and soon displaced much of the dolomite. With the extensive development of basic steel-melting, the rise of the copper industry, and other metallurgical and chemical processes which dealt with chemically basic substances, the use of magnesite grain and magnesite brick increased rapidly.

Jan 1, 1931

By James P. Savely, Victor L. Kastner

Inspiration Consolidated Copper Company is currently mining in four pit areas; Live Oak, Red Hill, Thornton and Joe Bush Extension, near Globe, Arizona. Small satellite orebodies lying outside the main pits have been mined out in a series of small open pits. Major slope instability has affected production in every pit. Some consequences of the instability have been; (1) Serious interruption of mining plans, which resulted in deferred ore production, lost ore, reduced mining rates and increased stripping requirements. (2) Forced replacement of crushing facilities. (3) Serious effects on other production facilities. The introduction of a slope stability monitoring and control function as an integral part of mine planning has been successful in reducing the impact of these failures and will eventually result in economic pit design based on probabilistic slope analysis. This case history presents a brief review of the problems associated with slope instability at Inspiration's mines followed by a more detailed report on one specific failure area in the Thornton pit where the use of horizontal drain holes for slope stabilization appears to be successful. Relationships between slope movement rate, rainfall, and mining activity are shown.

Jan 1, 1983

By J. A. Fellows, Earnshaw Cook, H. S. Avery

THE increased use of heat-resistant alloys (26 per cent Cr, 12 per cent Ni, 16 per cent Cr, 35 per cent Ni, 12 per cent Cr, 60 per cent Ni, etc ) in recent years has been accompanied by continued demands by the consumer for improvement in properties The manufacturers of these materials, of necessity, have resorted to more critical studies of the basic causes of variations in fundamental properties To keep pace with the need for augmented information, previous techniques of investigation have been refined and new test methods and instruments created It is the purpose of this paper to describe the apparatus, experimental technique and precision of measurement that were employed in the exploration of properties of heat-resistant alloy presented in a companion paper† The detailed precautions in experimental procedure essential for attainment of accurate and comparable data at elevated temperatures cannot be too highly emphasized THE CREEP TEST Since the fundamental concepts of creep testing have been recognized for the past 20 years, present interest is restricted to refinements in equipment and experimental procedure The creep-test laboratory constructed for the American Brake Shoe and Foundry Co is designed to permit 1000-hr tests in the temperature range of 1200° to 2200°F with a choice of applied stress extending from 50 to 50,000 lb per sq in in increments of 50 lb per sq in To simplify the calculation of weight combinations, the loading beams (Fig I) are provided with counterweights to eliminate the tare The precision of the knife-edges (10 1 ratio) is such that a 10-gram weight placed on the upper specimen grip will be exactly balanced by a 1-gram weight attached to the loading shackle Check of the loading weights proved the maximum error to be 0 06 per cent Axial alignment is provided by crossed knife-edges in the grip seats The furnaces are similar in design to those of Crane and Company, Battelle Memorial Institute, and the U S Steel Corporation An 80 per cent Pt, 20 per cent Rh No 19 B and S gauge wire is used as the heating element The details of construction are shown in the radiograph reproduced in Fig 2 The windings are held in place on an alundum tube with alundum cement, the distribution of turns is adjusted to give a maximum temperature gradient of ± 1°F over a 4-in gauge length (Fig 3) To avoid sharp temperature differentials at the ends of the test section, the length of the furnace is four times the gauge length Sixteen-inch coupons are used to reduce the temperature of the threaded

Jan 1, 1942

By C. S. Barrett, D. F. Clifton

THE transformation that occurs in lithium and its solid solutions containing magnesium1,2 is similar in many respects to other diffusionless transformations of the martensitic type. This general similarity makes it desirable to investigate the transformation curves in detail. The current interest in the phenomenon of stabilization in martensitic transformations has created a need for a careful appraisal of possible stabilization effects in both cooling and heating transformations in lithium alloys. The effect of prior heat treatment on the temperature at which transformation begins and the effect of various temperature cycles in partially transformed alloys also merit attention. Limited data on some of these features were presented previously,' but the present studies have been made with improved apparatus, in which erratic fluctuations were smaller than in the earlier work, and include many independent determinations of certain critical observations. Material and Methods Geiger counter X-ray spectrometers were used: a Norelco instrument, original model, and a General Electric XRD-3. The low-temperature specimen holder has been described elsewhere." Specimens 10 mm in diam and 1.5 mm thick were held in firm contact with a copper block which was attached to the lower end of a stainless steel tube that extended up to a reservoir of liquid nitrogen. A heating coil on the tube permitted a controlled temperature gradient along the tube, so that desired temperatures and rates of heating and cooling could be obtained by controlling the heating current. The specimen was surrounded by an atmosphere of evaporated nitrogen in an insulated chamber having double cellophane windows. The temperature of the specimen was read by a thermocouple imbedded in it close to the irradiated area; the specimen could be held at constant temperature within 1°C for long periods. The body-centered cubic 200 reflection near 8 = 26" was used as the index of the amount of b.c.c. material present; occasional checks were made using the most suitable line of the low-temperature phase, the close-packed hexagonal 110 line near 8 = 29". Copper radiation was used throughout. A continuous record was made of the reflected intensities on a strip chart recorder, both when the peak intensity of a line was being followed and when the lines were being scanned at constant temperature. On the continuous recordings of peak intensity, periodic checks were made on the background intensity between the lines, and on the setting of the spectrometer for maximum intensity. The lithium-base solid solution containing 12.4 atomic pct Mg (33.3 wt pct) that had been used previously' was chosen, as it had a transformation range at relatively high temperatures, so as to permit wide temperature cycling within the range. Just prior to use a pellet was cut from the ingot,

Jan 1, 1951

By G. M. Willis, F. L. Hennessy

The oxygen pressure in equilibrium with silver and Ag2O-B2O3 melts has been measured between 800' and 900°C, to obtain the thermodynamic properties of the liquid. The compound Ag20. 4B20:1 appears to exist in the liquid, which shows marked heat content and entropy effects. A KNOWLEDGE of the thermodynamic properties of binary liquid silicates, borates, and phosphates would be of considerable assistance in the interpretation of the behavior of multi-component metallurgical slags. However, the literature contains comparatively few studies of the thermodynamics of binary slags. The system Ag20-B,O, attracted our attention as it was known to give a single liquid phase,',' in which high contents of silver could be obtained (up to 61 pct Ag according to Foex2). Further, it would be expected that the partial pressure of oxygen over melts in equilibrium with metallic silver could be used to determine the activity of Ag2O in the Ag,O-B,O, system. In many respects, it may be expected that the reaction of a basic oxide with boric oxide would be analogous to its reaction with silica. Liquid immiscibility frequently occurs in both borate and silicate systems. With B2O3 and SiO reaction with a basic oxide presumably involves a breakdown of the three-dimensional network of the acid oxide by reaction with oxygen atoms common to more than one silicon or boron atom. Ag2O-B2O3 was therefore investigated as a model of a slag system in the hope that its thermodynamic properties would assist in understanding those of other systems. Several methods for determining the activity of a component in a slag have been described in the literature. Chang and Derge" used high temperature electromotive force measurements to obtain the activity of SiO2 in CaO-SiO2 and Ca0-Al203-Si02 slags, but the cell reaction in their work is not clear. low has used rate of volatilization and vapor pressure measurements combined with phase diagrams to obtain activities in the systems KO-SiO,, Na,O-SiO, and Li,O-SiO," and PbO-SiO26 Taylor and Chipman7 extrapolated their results for the distribution of FeO between liquid iron and CaO (+Mg0)-FeO-SiOl slags to obtain the activity of FeO in the binary FeO-SiO2 system. In principle, one of the most direct methods for obtaining the activity of a metallic oxide in a phase is by comparison of the equilibrium oxygen pressure for the system metal-pure oxide with that of metal oxide-containing phase. Schenck and othersa have studied the stabilization of Ag2O on combination with other oxides (MO,) in the solid state by measurements of the oxygen pressure in systems of the type Ag-Ag,O-xM0,-MOy-0, (gas). Schuhmann and Ensio" have determined the activity of FeO in iron silicate slags in equilibrium with solid iron, using CO/CO2 mixtures to establish known partial pressure of oxygen. Although the method gives the activity of FeO without ambiguity, the slag is not a binary system, and interpretation of the results in terms of the hypothetical binary system FeO-SiO, is not possible. If a metal is solid at temperatures at which the properties of the slag containing its oxide are to be studied, this method has the considerable experimental advantage that the metal can be used as the container for the slag, and contamination by contact with refractories is avoided. In this work, crucibles for Ag2-B,O, melts were made from silver, and the liquid brought to equilibrium with definite pressures of oxygen gas. The oxygen pressure PO, thus fixes the activity of Ag20 in the liquid silver borate. For the reaction at a given temperature. is substantially constant, is directly proportional to the square root of the equilibrium oxygen pressure. Varying the oxygen pressure changed the silver oxide content of the liquid and it was possible to obtain the activity of Ag2O over a range of composition. Experimental Procedure In principle, the method consisted of bringing melts in silver crucibles or boats to equilibrium at a fixed temperature under a definite pressure of oxygen and analyzing the glass after solidification. Materials: B2O3 glass was prepared from A.R. quality boric acid by fusion in platinum. The silver

Jan 1, 1954

By G. R. Speich

The age-hardening of Fe-18 to 21 pct Ni marten-sites containing small amounts of titanium, aluminum, copper, or molybdenum has been studied by hardness measurements, transmission electron microscopy, extraction replicas, and X-ray and electron diffraction. Electyon-probe microanaly-sis of the extracted precipitates was also performed. The effects of temperature and composition on the aging kinetics have been studied in detail for Fe-20 pctNi-Ti martensites. All the martensites hardened on aging at 400" to 500 "C with a single aging peak. In the Fe-20 pct Ni-Ti martensites hardening was associated with the formation of a fine dispersion of NisTi. No precipitation was observed in an Fe-21 pct Ni-2.6 pct A1 alloy, although the hardness increased from 327 to 545 Dph during aging at 500°C. Copper was precgitated from an Fe-20 pct Ni-10.7pct Cu alloy, at least during the later stages of age-hardening. Hardening in an Fe-18 pctNi-5pct Mo alloy was associated with the precipitation of an intemzetallic compound tentatively identified as NisMo. The formation of austenite and the recovery of the defect structure of the martensite occur simultaneously with the normal precipitation processes &ring aging of these alloys. THE age-hardening of substitutional iron-base martensites is an important subject for study since age-hardening is one of the principal means of strengthening the substitutional iron-base martensites in precipitation-hardening stainless steels1 and maraging steels.a~4 In contrast to Fe-C martensites, these martensites are relatively soft and ductile in the as-quenched condition, due to the low solid-solution hardening effect of the substitutional elements as compared to carbon. Also, these martensites are hardened by aging at low temperatures in contrast to Fe-C martensites which generally soften on tempering. Titanium and aluminum, singly or in combination, as well as copper and molybdenum, have been the principal alloying additions to stainless steels to obtain an age-hardening reaction.' Ti-A1 or Co-Mo-Ti combinations have been used in the case of maraging steels.3"4 The present work has been confined to a study of the age-hardening characteristics of an Fe-18 to 21 pct Ni martensite to which small amounts of titanium, aluminum, copper, and molybdenum were added in order to study the effects of each alloying element separately. The age-hardening characteristics of these alloys were studied by hardness measurements, transmission electron microscopy, extraction replicas, and X-ray and electron diffraction. Electron-probe micro-analysis of the extracted precipitates was also performed. The types and dispersion of precipitates, the formation of austenite, and the recovery of the defect structure of the martensite all were studied. EXPERIMENTAL PROCEDURE Alloys. The compositions of the alloys studied are listed in Table I. The level of 18 to 21 pct Ni was chosen to assure complete transformation to martensite on quenching and is the same nickel level used in maraging steels. The concentrations of titanium, aluminum, copper, and molybdenum were chosen after a study of the and Fe-Ni-MO' ternary diagrams indicated how much of each alloying element could be dissolved in austenite. Alloys with 2 and 4 pct Cu were also studied, but these did not show precipitation hardening at the nickel levels studied and will not be discussed further. The alloys were prepared from electrolytic iron and high-purity* nickel, titanium, aluminum, copper, and molybdenum by vacuum melting of 20-lb heats. These were vacuum-cast into two 8-lb ingots. The ingots were hot-rolled at 1100°C to 1/2-in. plate and subsequently cut into 3/8-in. cubes. The cubes were sealed in evacuated quartz capsules and solution-treated for 16 hr at 1100°C, except for the Fe-20 pct Ni-10.7 pct Cu alloy and Fe-21 pct Ni-2.6 pct A1 alloys which were solution-treated for 16 hr at 1300" and at 1250"C, respectively. Metallographic examina-

Jan 1, 1963

By M. C. Flemings, F. R. Mollard

Two-phase Pb-Sn alloys, ranging in compositiotz from 12 to 26 at. pct Pb, were unidirectionally solidified in a convection-fvee system, with thermal gradients in the liquid of up to 480°C per cm. Plane front solidification Loas achieved in all alloys at sufficiently steep gradient and slow growth rate. Conditions causing breakdown of the interface to a cellular or dendritic structure were roughly as predicted by a sinlple constitutional supercooling criterion. Structures of alloys of near-eutectic composition, solidified with plane front, exhibited a lamellar structure; the alloys furthest from the eutectic exhibited a rod-like morphology. Assumptions used in a previous paper for calculations of solute redistribution in two-phase plane front growth are shown to be reasonable for Pb-Sn alloys. Results of calculations are in good agveement with experiment. These show that variations in growth rate during solidification of the composite produce marked changes in average composition of the solid. IN a previous paper, Part I,' conditions necessary for plane front solidification of two-phase alloys were discussed and calculations given on solute redistribution in this type of solidification. This paper, Part 11, describes experiments on Pb-Sn alloys, designed to check the assumptions of the analyses presented, and to demonstrate their applicability to a given alloy system (Pb-Sn). APPARATUS AND PROCEDURE General. A vertical crystal growing unit was built for the study as described below, and "normal solidification" employed throughout (i.e., the ingot was completely melted except for a portion near the bottom end and then solidification initiated). The furnace was designed to permit achieving very low interface velocities, and steep gradients, in essential absence of convection; it is sketched in Figs. 1 and 2. Simple heat flow considerations indicated choice of a small-diameter specimen (ingot) to achieve high thermal gradients; ingot size chosen was 0.3 cm in diam. The ingots were held inside silica tubes 0.06 cm wall thickness. The requirement for an essentially convection-free system was met by use of the vertical furnace with the heat source over the heat sink, as well as by use of the small diameter ingots. In addition, by selection of tin-rich Pb-Sn alloys, the diffusion boundary layer (lead-rich) was denser than the bulk liquid and would not cause convection. The only apparent driving force for convection in this system was the small transverse temperature gradient resulting from heat flow into the samples from the furnace. Such convection must have been small, however, since 1) no temperature fluctuations in the melt were noted in the recordings, which would have indicated turbulent convection, and 2) experimental results obtained and described below could not have been achieved in presence of significant convection. Ingot Preparation. Pb-Sn alloys ranging from 12 to 26 at. pct Pb were prepared from high-purity lead and tin (99.9999 pct pure metal). Each alloy was prepared by first melting the pure metals in the proper ratio in air, in a Pyrex container. The melt was then stirred thoroughly with a graphite rod and cast into a preheated graphite mold. Ingots were then prepared from these castings for use in the actual experiments; each ingot consisted of a rod of alloy, 15 cm long in a 25-cm-long transparent fused-silica tube, 0.3 cm ID and 0.06 cm wall thickness. One chromel-alumel thermocouple, made with 0.004-in.-diam wire and protected by a two-hole alumina tube, was inserted into each ingot. The 1.5 cm of the thermocouple nearest the bead were protruding from the alumina tube and were coated with a very thin layer of boron nitride paste which provided electrical insulation while allowing good heat conduction. The electrically welded junction size was about that of each wire and the cross section of the two wires represented about 0.3 pct of the sample cross section. Including the coating, the thermocouple cross section still represented less than 0.5 pct of the ingot cross

Jan 1, 1968